Determination of perfluorooctanoic acid and perfluorooctane sulfonate in cooking oil and pig adipose tissue using reversed-phase liquid–liquid extraction followed by high performance liquid chromatography tandem mass spectrometry

• PFOA and PFOS were analyzed in cooking oil and pig adipose tissue.
• A rapid and simple one-step reversed-phase liquid–liquid extraction was used for pretreatment.
• LC–MS/MS method was developed and validated for the analysis of PFOA and PFOS.
• The partition theory of PFOA and PFOS in extraction solution systems was discussed.
• This method has been successfully applied to the analysis of PFOA and PFOS in real samples.

Perfluorooctanoic acid (PFOA) and perfluorooctane sulfonic acid (PFOS) are two perfluorinated compounds (PFCs) ubiquitously present in the environment, which could pose potential adverse effects on human health. Contamination and presence of PFOA and PFOS should be eliminated or rigidly restricted in food stuffs such as cooking oils and lard (from pig adipose tissue). This work describes a rapid, simple, reliable and sensitive method for quantitative analysis of PFOA and PFOS in cooking oils and pig adipose tissue with liquid chromatography tandem mass spectrometry (LC–MS/MS). The pretreatment mainly included a one-step reversed-phase liquid–liquid extraction using the mixture of basified water/methanol as the aqueous system, and dichloromethane (DCM) as the non-polar system. PFOA and PFOS can be successfully separated from the two lipid-rich matrices, i.e., cooking oil and adipose tissue, and extracted into the aqueous system, and then directly analyzed with LC–MS/MS. This method was validated in terms of accuracy (both intra- and inter-batch), precision, recovery, linearity, sensitivity and applicability. The intra-batch accuracies for PFOA and PFOS in cooking oil samples were within 93.9–101.9% with relative standard deviation (RSD) no more than 10.9%, and the inter-batch accuracies were 91.2–96.2% with RSD not exceeding 10.0%. The intra-batch accuracies of the analytes in pig adipose tissue samples were 102.9–113.0% with RSD of 8.8–13.1%. And the quantification ranges of PFOA and PFOS were 0.01–25 ng/mL. This method has been applied to the analysis of PFOA and PFOS in real samples collected from local markets in Guangzhou, China.